US5206060A - Process and device for the deposition of thin layers and product made thereby - Google Patents

Process and device for the deposition of thin layers and product made thereby Download PDF

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Publication number
US5206060A
US5206060A US07/565,295 US56529590A US5206060A US 5206060 A US5206060 A US 5206060A US 56529590 A US56529590 A US 56529590A US 5206060 A US5206060 A US 5206060A
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United States
Prior art keywords
substrate
process according
deposition
layer
power lead
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Expired - Lifetime
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US07/565,295
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English (en)
Inventor
Pierre Balian
Jean-Paul Rousseau
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Saint Gobain Glass France SAS
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Saint Gobain Glass France SAS
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Assigned to SAINT GOBAIN VITRAGE INTERNATIONAL reassignment SAINT GOBAIN VITRAGE INTERNATIONAL ASSIGNMENT OF ASSIGNORS INTEREST. Assignors: BALIAN, PIERRE
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    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
    • C23C16/50—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating using electric discharges
    • C23C16/505—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating using electric discharges using radio frequency discharges
    • C23C16/509—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating using electric discharges using radio frequency discharges using internal electrodes
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
    • C03C17/34—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions
    • C03C17/36—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions at least one coating being a metal
    • C03C17/38—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions at least one coating being a metal at least one coating being a coating of an organic material

Definitions

  • This invention relates to a process and a device for depositing a thin layer using a plasma-CVD technique on a conductive substrate where the substrate itself is used as an electrode for an electrical current.
  • a plasma-CVD technique on a conductive substrate where the substrate itself is used as an electrode for an electrical current.
  • an insulating substrate can be used that is first made conductive by the deposition of a thin conductive layer.
  • the thin conductive layer will remain intact when the final product is obtained.
  • the invention also relates to a substrate covered by thin layers including at least one metal layer, preferably silver, on which a layer such as an organosilicon layer is deposited according to the process of the invention.
  • the substrate remains immobile during the deposition.
  • the plasma is contained with a magnetic field and the substrate is displaced relative to the electrodes and therefore relative to the plasma.
  • this process also has its limits. It has been observed that the zone where the major portion of the polymer deposition is performed is that closest to the electrode located above the substrate. Additionally, the deposition is performed as quickly on the upper electrode as on the substrate to be treated. This has multiple negative consequences. First, the quantitative efficiency of the process is low since only a small proportion of the monomers introduced in the chamber are found in the polymer on the glass. Furthermore, the operation of the process itself is impeded by the preferred deposition on the upper electrode because the deposition, which is insulating, modifies the characteristics of the electrical field created under the electrode. This in turn creates a drift that must be corrected by adjusting the electrical parameters of the process. Additionally, a harmful mechanical effect can also be manifested when several glass sheets are treated successively.
  • the deposition on the electrode increases in thickness as the successive sheets are treated; and the thickening layer becomes friable and eventually disintegrates. Chips then fall on the substrate where they disturb the deposition process. Further, the rate of deposition on the glass is not very high and the thickness of the final layer is greater at the center than it is opposite the edges of the electrode.
  • An object of this invention is to eliminate these various drawbacks.
  • a thin layer is deposited by a plasma-CVD technique on a conductive substrate where the substrate itself is used as an electrode to create the discharge.
  • the substrate consists of an insulating material covered by a thin conductive layer.
  • the deposition is performed up to 180 cm from the power lead-in and preferably up to about 160 cm. Moreover, the frequency is advantageously between 10 and 400 kHz. When the deposition is of an organosilicon compound, it is performed in the presence of oxygen supplied by nitrous oxide.
  • the invention also relates to the product formed by this process, namely a substrate covered by thin layers including at least one metal layer, in particular silver, on which a thin layer such as an organosilicon layer is deposited.
  • FIG. 1 shows a diagrammatic view of an illustrative installation utilizing the process of the present invention
  • FIG. 2 shows a power lead-in which delivers current to a conductive substrate
  • FIG. 3 depicts experimental conditions which make it possible to make the deposition at a great distance from the power lead-in of FIG. 2.
  • FIG. 1 diagrams the installation.
  • a vacuum chamber 1 is evacuated utilizing a pipe 2 which is connected to a primary and/or secondary conventional pumping system, not shown.
  • a valve 3 makes it possible to separate the installation from the pumps. This is particularly useful when it is desired to link the inside of the chamber with the ambient atmosphere.
  • Gas is introduced into chamber 1 through pipe 6 under control of valve 7 which is regulated by a gas managment system (not shown).
  • a substrate 4 covered by a conductive layer 5 is located within chamber 1.
  • At least one power lead-in 8 is used to connect the substrate to an alternating voltage source 9 (FIG. 1) by a suitable cable 10.
  • the chamber itself is grounded by a cable 11 as is a second pole 12 of alternating current source 9.
  • the power lead-in itself is placed over the entire length of the edge of substrate 4. It comprises a conductive element 13, copper in the example, which is surrounded by an insulating material 14 on all sides except the side in contact with layer 5.
  • FIG. 2 shows a detailed view of a particular embodiment of power lead-in 8.
  • Power lead-in 8 comprises two blocks 15, 16 of an insulating material 14 such as PTFE. These two blocks are connected together and clamped onto substrate 4, by bolts 17.
  • a copper conductor 13 is mounted in block 15 and extends all along the edge of sheet 4 in contact with conductive layer 5.
  • Conductor 13 is itself pressed to conductive layer 5 by a series of insulating bolts 18 and it is connected by cable 10 to alternating current source 9.
  • substrate 4 is a glass sheet covered by a conductive layer 5 which consists, for example, of a layer of silver that is 10 nm thick deposited between two layers of tin oxide (SnO 2 ), each 40 nm thick.
  • a conductive layer 5 which consists, for example, of a layer of silver that is 10 nm thick deposited between two layers of tin oxide (SnO 2 ), each 40 nm thick.
  • SnO 2 tin oxide
  • These layers are relatively sensitive to outside influences; and silver, in particular, is a mechanically and chemically fragile metal.
  • the layer is formed by introducing a mixture of a plasma-generating gas and an organosilicon monomer such as, for example, hexamethyldisiloxane (HMDSO) or hexamethyldisilazane (HMDS) and, in general, alkylsilazanes, vinyltrimethoxysilane (VTMOS), vinyldimethylethoxysilane (VDMEOS), dimethyldiethoxysilane (DMDEOS), trimethylethoxysilane (TMEOS), tetramethoxysilane (TMOS), tetraethoxysilane (TEOS) and, in general, alkoxysilanes, into an electrical discharge within a chamber as discussed below.
  • HMDSO hexamethyldisiloxane
  • HMDS hexamethyldisilazane
  • VTMOS vinyltrimethoxysilane
  • VDMEOS vinyldimethylethoxysilane
  • DMDEOS dimethyldie
  • the process of this invention also works for other gases making it possible to obtain layers of different materials.
  • methane gas can be used to produce a carbon layer or an organometallic can be used to produce a layer whose main component is the oxide of the metal concerned.
  • the process of this invention also works for other conductive layers such as Al, Ti, Ta, Cr, Mn, Zr and Cu, as well as for multiple conductive layers. Additionally, the conductive layer can be entirely omitted where a conductive substrate is employed.
  • the monomer proportion in the plasma-generating gas depends on the respective natures of the gases used and the conditions of the deposition. The conditions of the following example provide good results.
  • a cylindrical chamber having a vertical axis of a height of 35 cm and a diameter of 60 cm.
  • the sample was of a plane window glass 4 mm thick made of a soda-lime-silica glass with dimensions of 30 ⁇ 30 cm.
  • This window glass was covered by a triple layer comprising a dielectric underlayer of SnO 2 , 40 nm thick deposited by reactive cathode sputtering from a tin target; an "active" layer of silver, 10 nm thick deposited by the same method in an argon atmosphere; and a third dielectric layer similar to the first.
  • This covered glass was placed at the midheight of the chamber with its layered side facing upward and resting on a suitable support.
  • the deposition technique requires a particularly clean substrate. This can be achieved by carefully cleaning the substrate or by performing the deposition immediately following the deposition of the underlying layers without returning to the atmosphere.
  • the cleaning advantageously is ended by a discharge.
  • argon is introduced and the pressure is then allowed to increase to 0.40 hPa.
  • a discharge is then created with an alternating current that is established between the conductive surface of the substrate and the chamber with a frequency of 100 kHz and a power of 100 watts. After 30 seconds, the current is turned off.
  • the protective layer is deposited by introducing a monomer gas which is carried by the plasma-generating gas.
  • the plasma-generating gas was the nitrous oxide N 2 O, which supplied the oxygen necessary for the reaction.
  • Tests with an argon-oxygen mixture have also been fully satisfactory.
  • the organosilicon gas in the experiment was hexamethyldisiloxane (HMDSO) in a proportion of 10%. After the vacuum pressure was stabilized at 0.15 hPa, the mixture was introduced with a delivery of 200 cm 3 /mn (standard temperature and pressure (STP)).
  • the plasma is ignited by applying an alternating voltage to conductor 13.
  • the frequency was 100 kHz and the best results were obtained with a power of 300 watts for a power lead-in length of 30 cm.
  • Tests showed that, in a general, the deposition conditions were comparable if the power varied proportionally to the length of the power lead-in. In the case of the example, a homogeneous and regular layer 30 nm thick was obtained in 8 seconds.
  • the deposition occurs all along track 20 up to and including farthest zone 22. Its thickness is regular, with a thickness of 20 ⁇ 2 nm being measured. These thickness variations are virtually undetectable by the eye.
  • the process makes it possible to obtain quality depositions at large distance, i.e., in the order of at least 180 cm, from the power lead-in. If two power lead-ins are used, each on one of the two opposite sides of a substrate of float glass coated by a conductive layer, the technique makes it possible to deposit a layer by plasma-CVD on a typical industrial plate such as those having a width of 3.20 m or 4.00 m.
  • the process of the invention provides a very advantageous technique to produce layers.
  • thin organosilicon layers of good quality can be formed on substrates which are conductive or made conductive due to the prior deposition of conductive layers.
  • This technique is compatible with the industrial production of large layered glass plates particularly those in which an underlayer is deposited on a glass already equipped with a conductive layer, for example, by pyrolization, or an over layer, before or after the deposition of dielectric and/or metallic layers by cathode sputtering.
  • This process is then performed preferably in the input or output lock chamber of an industrial production line.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Metallurgy (AREA)
  • Mechanical Engineering (AREA)
  • Physics & Mathematics (AREA)
  • Plasma & Fusion (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Chemical Vapour Deposition (AREA)
  • Glass Compositions (AREA)
  • Light Receiving Elements (AREA)
  • Superconductors And Manufacturing Methods Therefor (AREA)
US07/565,295 1989-08-14 1990-08-09 Process and device for the deposition of thin layers and product made thereby Expired - Lifetime US5206060A (en)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
FR8910870A FR2650822B1 (fr) 1989-08-14 1989-08-14 Procede de depot de couches minces
FR8910870 1989-08-14

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US (1) US5206060A (ja)
EP (1) EP0413617B1 (ja)
JP (1) JP3165143B2 (ja)
AT (1) ATE120439T1 (ja)
DE (1) DE69018159T2 (ja)
ES (1) ES2071055T3 (ja)
FR (1) FR2650822B1 (ja)

Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5354583A (en) * 1992-11-09 1994-10-11 Martin Marietta Energy Systems, Inc. Apparatus and method for selective area deposition of thin films on electrically biased substrates
WO1995023652A1 (en) * 1994-03-03 1995-09-08 Diamonex, A Unit Of Monsanto Company Ion beam process for deposition of highly abrasion-resistant coatings
US5571571A (en) * 1993-06-16 1996-11-05 Applied Materials, Inc. Method of forming a thin film for a semiconductor device
WO1997038850A1 (en) * 1996-04-15 1997-10-23 Monsanto Company Highly durable and abrasion-resistant dielectric coatings for lenses
US5888593A (en) * 1994-03-03 1999-03-30 Monsanto Company Ion beam process for deposition of highly wear-resistant optical coatings
US6077567A (en) * 1997-08-15 2000-06-20 University Of Cincinnati Method of making silica coated steel substrates
US6607790B1 (en) * 1993-04-13 2003-08-19 Applied Materials, Inc. Method of forming a thin film for a semiconductor device
WO2009077660A1 (en) * 2007-12-19 2009-06-25 Beneq Oy A glass product and a method for manufacturing a glass product
WO2013079798A1 (en) * 2011-12-01 2013-06-06 Beneq Oy Surface treatment apparatus and method
CN107056085A (zh) * 2017-06-08 2017-08-18 东莞鑫泰玻璃科技有限公司 一种烤箱用隔热玻璃及其制备方法

Families Citing this family (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
NO931606L (no) * 1992-05-26 1993-11-29 Saint Gobain Vitrage Vindusplate med en funksjonell film
FR2701474B1 (fr) * 1993-02-11 1995-03-31 Saint Gobain Vitrage Int Vitrage muni d'une couche fonctionnelle.
JP5015046B2 (ja) 2008-03-17 2012-08-29 株式会社リコー 情報処理装置及び情報処理方法

Citations (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4252837A (en) * 1976-03-23 1981-02-24 Warner-Lambert Company Blade shields
US4382100A (en) * 1976-08-13 1983-05-03 National Research Development Corporation Application of a layer of carbonaceous material to a surface
US4407852A (en) * 1979-10-19 1983-10-04 Sapieha Slawomir W Electrets from plasma polymerized material
US4508049A (en) * 1978-11-02 1985-04-02 Siemens Aktiengesellschaft Method and a device for the production of electrical components, in particular laminated capacitors
EP0154814A2 (en) * 1984-03-16 1985-09-18 American Cyanamid Company Substrates coated by plasma enhanced chemical vapor deposition, apparatus and process for their production
US4599266A (en) * 1982-06-18 1986-07-08 Tdk Corporation Magnetic recording medium
US4612207A (en) * 1985-01-14 1986-09-16 Xerox Corporation Apparatus and process for the fabrication of large area thin film multilayers
US4632844A (en) * 1984-02-04 1986-12-30 Japan Synthetic Rubber Co., Ltd. Optical product having a thin film on the surface
EP0230188A1 (fr) * 1985-12-17 1987-07-29 Saint-Gobain Vitrage International Film organo-minéral déposé sur un substrat en verre éventuellement revêtu d'une ou plusieurs couches métalliques minces
US4693927A (en) * 1984-03-19 1987-09-15 Fuji Photo Film Company Limited Magnetic recording medium and process for producing the same
US4762730A (en) * 1986-07-19 1988-08-09 Leybold-Heraeus Gmbh Method for producing transparent protective coatings from silicon compounds

Family Cites Families (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH01195285A (ja) * 1988-01-29 1989-08-07 Stanley Electric Co Ltd メタライズガラス基板の製造方法

Patent Citations (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4252837A (en) * 1976-03-23 1981-02-24 Warner-Lambert Company Blade shields
US4382100A (en) * 1976-08-13 1983-05-03 National Research Development Corporation Application of a layer of carbonaceous material to a surface
US4508049A (en) * 1978-11-02 1985-04-02 Siemens Aktiengesellschaft Method and a device for the production of electrical components, in particular laminated capacitors
US4407852A (en) * 1979-10-19 1983-10-04 Sapieha Slawomir W Electrets from plasma polymerized material
US4599266A (en) * 1982-06-18 1986-07-08 Tdk Corporation Magnetic recording medium
US4632844A (en) * 1984-02-04 1986-12-30 Japan Synthetic Rubber Co., Ltd. Optical product having a thin film on the surface
EP0154814A2 (en) * 1984-03-16 1985-09-18 American Cyanamid Company Substrates coated by plasma enhanced chemical vapor deposition, apparatus and process for their production
US4693927A (en) * 1984-03-19 1987-09-15 Fuji Photo Film Company Limited Magnetic recording medium and process for producing the same
US4612207A (en) * 1985-01-14 1986-09-16 Xerox Corporation Apparatus and process for the fabrication of large area thin film multilayers
EP0230188A1 (fr) * 1985-12-17 1987-07-29 Saint-Gobain Vitrage International Film organo-minéral déposé sur un substrat en verre éventuellement revêtu d'une ou plusieurs couches métalliques minces
US4762730A (en) * 1986-07-19 1988-08-09 Leybold-Heraeus Gmbh Method for producing transparent protective coatings from silicon compounds

Cited By (17)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5354583A (en) * 1992-11-09 1994-10-11 Martin Marietta Energy Systems, Inc. Apparatus and method for selective area deposition of thin films on electrically biased substrates
US6607790B1 (en) * 1993-04-13 2003-08-19 Applied Materials, Inc. Method of forming a thin film for a semiconductor device
US5571571A (en) * 1993-06-16 1996-11-05 Applied Materials, Inc. Method of forming a thin film for a semiconductor device
WO1995023652A1 (en) * 1994-03-03 1995-09-08 Diamonex, A Unit Of Monsanto Company Ion beam process for deposition of highly abrasion-resistant coatings
US5508368A (en) * 1994-03-03 1996-04-16 Diamonex, Incorporated Ion beam process for deposition of highly abrasion-resistant coatings
US5846649A (en) * 1994-03-03 1998-12-08 Monsanto Company Highly durable and abrasion-resistant dielectric coatings for lenses
US5888593A (en) * 1994-03-03 1999-03-30 Monsanto Company Ion beam process for deposition of highly wear-resistant optical coatings
US6077569A (en) * 1994-03-03 2000-06-20 Diamonex, Incorporated Highly durable and abrasion-resistant dielectric coatings for lenses
USRE37294E1 (en) 1994-03-03 2001-07-24 Diamonex, Incorporated Ion beam process for deposition of highly abrasion-resistant coatings
WO1997038850A1 (en) * 1996-04-15 1997-10-23 Monsanto Company Highly durable and abrasion-resistant dielectric coatings for lenses
US6077567A (en) * 1997-08-15 2000-06-20 University Of Cincinnati Method of making silica coated steel substrates
WO2009077660A1 (en) * 2007-12-19 2009-06-25 Beneq Oy A glass product and a method for manufacturing a glass product
CN101945832A (zh) * 2007-12-19 2011-01-12 贝尼科公司 一种玻璃制品以及制造玻璃制品的方法
EA016639B1 (ru) * 2007-12-19 2012-06-29 Бенек Ой Стеклянное изделие и способ изготовления стеклянного изделия
WO2013079798A1 (en) * 2011-12-01 2013-06-06 Beneq Oy Surface treatment apparatus and method
CN107056085A (zh) * 2017-06-08 2017-08-18 东莞鑫泰玻璃科技有限公司 一种烤箱用隔热玻璃及其制备方法
CN107056085B (zh) * 2017-06-08 2023-09-05 东莞鑫泰玻璃科技有限公司 一种烤箱用隔热玻璃及其制备方法

Also Published As

Publication number Publication date
FR2650822B1 (fr) 1993-01-08
ES2071055T3 (es) 1995-06-16
FR2650822A1 (fr) 1991-02-15
EP0413617A1 (fr) 1991-02-20
JPH03183781A (ja) 1991-08-09
ATE120439T1 (de) 1995-04-15
JP3165143B2 (ja) 2001-05-14
DE69018159T2 (de) 1995-10-26
DE69018159D1 (de) 1995-05-04
EP0413617B1 (fr) 1995-03-29

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